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目的建立去痛片中氨基比林、非那西丁、咖啡因和苯巴比妥的超高效液相色谱(UPLC)分析方法。方法将供试品用流动相超声提取,采用Waters ACQUITY UPLC BEH C18色谱柱(2.1 mm×100 mm,1.7μm),以0.05 mol/L磷酸二氢钾溶液-甲醇(55∶45,V/V)为流动相,检测波长为214 nm,流速为0.2 ml/min,柱温为30℃,进样体积为5μl。外标法峰面积定量。结果 4种成分在4 min内完成分离,线性范围为0.6μg/ml~210μg/ml,标准曲线的线性关系良好,相关系数(r)为0.999 2~0.999 5。检出限(S/N=3)为0.012 6 ng~0.035 7 ng,平均回收率为97.0%~100.3%,RSD为1.15%~1.55%。2批样品含量测定结果均符合国家标准规定。结论经验证,该方法简便、快速、分离效果好、灵敏度高,准确性和稳定性好,在日常检测中可大大降低检测成本,缩短检测周期,适用于去痛片中4种成分的含量测定。
Objective To establish a method for the determination of aminopyrine, phenacetin, caffeine and phenobarbital in painkiller tablets by UPLC. Methods The samples were extracted with mobile phase by ultrasonic. The mobile phase was eluted with 0.05 mol / L potassium dihydrogen phosphate solution - methanol (55:45, V / V) using a Waters ACQUITY UPLC BEH C18 column (2.1 mm × 100 mm, ) As the mobile phase, the detection wavelength was 214 nm, the flow rate was 0.2 ml / min, the column temperature was 30 ℃ and the injection volume was 5μl. External standard peak area of quantitative. Results The four components were separated within 4 min. The linear range was 0.6μg / ml ~ 210μg / ml. The calibration curve showed a good linear relationship with a correlation coefficient (r) of 0.999 2-0.9995. The detection limit (S / N = 3) was 0.012 6 ng 0.035 7 ng with average recoveries of 97.0% -100.3% and RSD 1.15% -1.55%. 2 batches of sample content determination results are in line with national standards. Conclusion The method has been proved to be simple and rapid with good separation effect, high sensitivity, good accuracy and stability. It can greatly reduce the testing cost and shorten the test period in daily test, which is suitable for the determination of four components .